Method and composition for delustering artificial silk



Patented Dec. 11, 1945 I METHOD AND COMPOSITION FOR DE- LUSTERING ARTIFICIAL SILK Jesse Werner, Brooklyn, N. Y., assignor to General Aniline & Film Corporation, New York, N. Y., a corporation of Delaware No Drawing. Application September 26, 1944,

' Serial N0. 555,893

Claims.

The present invention relates to the. dulling or matting of artificial silk and particularly to a composition for matting or dulling artificial silk by a one bath process.

It has been proposed to mat or dull artificial silk by treating the same in a oneor two-bath process with a. composition containing a pigment and a binding agent for the pigment. Various binding agents have been mentioned in the literature, and among those suggested have been derivatives of big'uanide. The art, however, has always been under the impression that when using these substances as binding agents they pigments will be carried onto and adhesively retained by the fibers. In this connection, reference is made to U. S. Patents 2,123,987 and 2,185,427. The earlier patent proposes inter alia as the binding agent, water-soluble salts of biguanides in which the biguanide is substituted by an alkyl chain or at least 10 carbon atoms. The patent mentions as examples of such commust be water soluble in order to insure that the pounds, dodecyl biguanide hydrochlorideand' ste'aryl biguanide hydrochloride. The later patent proposes to use salts of biguanides having a long alkyl chain and which have been polyvention to provide delustering compositions containing a pigment and a water-insoluble free biguanide base containing an alkyl chain of at least 10 carbon atoms.

A further object of the invention is-a process of delustering artificial silk in a one-bath process by subjecting the silk to the action of a composition comprising a pigment and a water-insoluble free biguanide base containing an alkyl chain of at least 10 carbon atoms.

Other objects of the invention will be apparent as the description proceeds.

Any of the pigments previously employed by the art may be utilized for my purpose. Such pigments include zinc sulfide, titanium dioxide,

'lithopone, barium sulfate, china clay, and the like.

The biguanide derivative which must be water insoluble is, as previously stated, a biguanide containing in its molecule an alkyl chain of at least 10 carbon atoms. Biguanide derivatives of this character which are efiective for my purposes are decyl biguanide, dodecyl biguanide,

, stearyl biguanide, oleyl biguanide and-the like.

hydroxyethylated by treatment with ethylene oxide. It is emphasized that this treatment makes the biguanide derivatives more soluble than the salts mentioned in the earlier patent.

I have now found that contrary to expectation, compositions superior to those mentioned in the patents are produced if there be utilized for the binding agent a water-insoluble free biguanide base (in contradistinction to the salts of such bases), the base containing an alkyl chain of at least 10 carbon atoms. why the water-insoluble base gives superior compositions is not known. It would logically appear that the water-soluble products would operate more effectively, since they would appear to insure a better absorption of the pigments and binding agents by the fibers, and it was undoubtedly for this reason that previous proposals suggested that the biguanide derivatives employed be water-soluble. Irrespective, however. of the theory involved, it is a fact that when utilizing the water-insoluble free base in lieu of water-soluble salts or water-soluble derivatives of the salts, compositions are obtained which are far superior in dispersibility, stability after dilution with water and delustering power and which do not cause any changes in color of the dyestuil's in the material treated.

The particular reason It is to be emphasized, however, that any of the water-insoluble biguanides containing said lon alkvl chain are efiicacious. However, the stearyl biguanide gives best results and is to be preferred.

It is preferable to incorporate in the compositions a wetting or dispersing agent. Any of the usualwetting or dispersing agents may be employed, such as the alkylated naphthalene sulionic acids, aminocarboxylic and sulfonic acids in which the nitrogen atom is acylated with a long-chain fatty acid, alcohols having 10 carbon atoms and more, the carbon chains of which may I be interrupted by one or more hetero atoms or atom groups, for instance, O--, 000- and hols, amines and the like with ethylene oxide, ethers and esters of such conversionproducts which contain free hydroxyl groups, esters and amides of soap-forming fatty acids containing free hydroxyl groups, and the like. Examples of such products, are: diisobutylnaphthalene sulfonic acid, N-stearoyl sarcosine, N-stearoyl glycine, stearic acid mono-glyceride, oleyl polyglycol ether, stearyl polyglycol ether, stearlc acid polyglycol or polyglycerol ester, lauric acid monoglycol ester and palmitic acid mono-ethanol amide. f

The amounts'of the various agents which go to make upthe compositions may vary to a large extent. The quantity ofpigment to biguanide It is accordingly an object of the present inderivative will usually range from 8 to 25 parts of pigment to one part of the biguanide base. The wetting agent is used in an amount which is a fraction of that of the biguanide base. Amounts of wetting agents which are found to be suitable range from one part oi wetting agent for about each 2 to 25 parts of the biguanide base.

The compositions may be compounded in various ways. Thus, the biguanide in the dry state may be added to water and the resulting mixture milled in a ball mill or a similar device. On theother hand, the wetting agent may be incorporated during the manufacture of the biguanide base and the resulting mixture subsequently milled with the pigment and water. The pigment, biguanide base and wetting agent may also be milled in the dry condition and stored and shipped as a dry composition. The water which is to be added to the compositions when they are to be utilized for dulling or matting will be in an amount to give a dispersion which will permit ready processing of the artificial silk.

Example 1 2600 parts of zinc sulfide, Boo parts of stearyl biguanide, parts of oleyl polyglycol ether, and 1080 parts of water are ball milled for 24 hours. The resulting composition is then run through a homogenizer. The product after diluting withwater is very stable and has a dispersibility afar exceeding that of similar compositions in which a water-soluble salt of stearyl biguanide or similar water-soluble compounds are employed.

A composition is prepared by dispersing 1 gram of the above composition in 1 liter of water. Lustrous. viscose silk is subjected to the action of fifty times its weight of such a composition for one-half hour at a temperature of about C. The silk is thereby given a matt efiect which is far superior to that obtained when utilizing a water-soluble stearyl biguanide.

Similar results are obtained when the viscose silk is replaced by a mixed fabric of 80 parts of wool and 20 parts of viscose artificial silk.

Esample 2.

with the stearyl biguanide hydrochloride to convert the same to the water-insoluble free base. 2600 parts of zinc sulfide are now added and the mixture ball milled for 24 hours. The resulting composition is run through a homogenizer and upon dilution with water a product is obtained which is exceedingly stable. 'It has a dispersibility and delu'stering power equivalent to the composition of Example 1.

Compositions having the properties 01 Examples 1 and 2 are also obtained it the stearyl biguanide in Examples 1 and 2 are replaced by dodecyl biguanide, oleyl biguanide, decyl biguanide, and the like.

. Various modifications of the invention wil1 occur to the worker skilled in the art and I accordingly do not intend to be limited in the patent granted except as required by the prior art and the accompanying claims.

I claim:

1. A composition for matting or delustering artificial silk comprising a pigment and a waterinsoluble free biguanide base containing an alkyl chain of at least 10 carbon atoms.

- 2. A composition for matting or delustering artificial silk comprising an aqueous suspension oi. a pigment and a water-insoluble free biguanide .base containing an alkyl chain of at least 10 carbon atoms.

3. A composition for matting or delustering artificial silk comprising anaqueous suspension of a pigment, a wetting agent and a water-insoluble iree biguanide base containing an alkyl chain of at least 10 carbon atoms.

4. A composition for matting or delustering artificial silk comprising an aqueous suspension of zinc sulfide, stearyl biguanide, and a wetting agent.

. 5. The composition as defined in claim 4 in which the Wettingv agent is a hydroxy polyethenoxy compound containing a long alkyl chain. 6.-The process of matting or delustering artificial silk which comprises subjecting the silk to the action of an aqueous suspension of a pigment and a water-insoluble tree biguanide base containing an alkyl chain of at least 10 carbon atoms. 1

. 7. The process of matting or delustering artificial silk which comprises subjecting the artificial silk to the action of an aqueous suspension of a pigment, a water-insoluble free biguanide base containing an alkyl chain of at least 10 carbon atoms and a wetting agent.

8. The process as defined in claim 7 wherein the pigment is zinc sulfide, the biguanide base is stearyl biguanide, and the wetting agent is a hydroxy polyethenoxy compound containing a long alkyl chain.

9. A composition for matting or delustering artificial silk comprising an aqueous suspension of zinc sulfide, stearyl biguanide and oleyl polyglycol ether.

10. The process of matting or delustering artificial silk which comprises subjecting the artificial silk to the action oi. an aqueous suspension of zinc sulfide, stearyl polyglycol ether.

, JESSE WERNER.

biguanide and oleyl 

